Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis - SC, Brazil.
Talanta. 2011 Oct 15;85(5):2681-5. doi: 10.1016/j.talanta.2011.08.044. Epub 2011 Aug 30.
High-resolution continuum source molecular absorption of the calcium mono-fluoride molecule CaF in a graphite furnace has been used to determine fluorine in tea after acid digestion, alkaline solubilization and preparation of a conventional aqueous infusion. The strongest absorption 'line' of the CaF molecule is at 606.440 nm, which is part of the rotational fine structure of the X(2)Σ(+)-A(2)Π electronic transition; it has a bond dissociation energy of 529 kJ mol(-1), which is comparable with other molecules used for fluorine determination. One advantage of using Ca as the molecule-forming reagent is that spectral interferences are extremely unlikely in the spectral range of its strongest absorption. Another advantage is that Ca acts both as molecule forming reagent and chemical modifier, so that no other reagent has to be added, making the method very simple. The only disadvantage is that Ca has a somewhat negative influence on the graphite tube lifetime. The limit of detection was found to be 0.16 mg L(-1) F, corresponding to 1.6 ng F absolute, and the calibration curve was linear in the range between 0.5 and 25 mg L(-1) with a correlation coefficient of R=0.9994. The results obtained for a certified tea reference material were in agreement with the certified value on a 95% confidence level. There was also no difference between the results obtained after an acid digestion and an alkaline solubilization for 10 tea samples, based on a paired t-test. The values found in the 10 samples ranged between 42 μg g(-1) and 87 μg g(-1) F; the tea infusions contained between 21 μg g(-1) and 56 μg g(-1) F, with an extraction rate between 48% and 74%.
采用石墨炉中钙单氟化物(CaF)分子的连续光源高分辩率原子吸收光谱法,对经酸消解、碱融解并配制成常规水溶液后的茶叶中的氟进行了测定。CaF 分子最强的吸收“谱线”位于 606.440nm,它是 X(2)Σ(+)-A(2)Π 电子跃迁的转动精细结构的一部分;其键离解能为 529kJmol(-1),与用于氟测定的其他分子相当。选择 Ca 作为分子形成试剂的一个优点是,在其最强吸收的光谱范围内,光谱干扰极不可能发生。另一个优点是 Ca 既能作为分子形成试剂,又能作为化学改性剂,因此无需添加其他试剂,使方法非常简单。唯一的缺点是 Ca 对石墨管的寿命有一定的负面影响。检测限为 0.16mgL(-1)F,相当于 1.6ngF 绝对量,校准曲线在 0.5-25mgL(-1)范围内呈线性,相关系数 R=0.9994。对一种有证茶叶参考物质的测定结果与有证值在 95%置信水平上一致。对 10 个茶叶样品进行酸消解和碱融解后,基于配对 t 检验,结果没有差异。在 10 个样品中发现的氟含量范围为 42μg g(-1)至 87μg g(-1)F;茶浸提液中氟含量范围为 21μg g(-1)至 56μg g(-1)F,提取率为 48%-74%。